A novel technique for assay of thermal and fast neutrons in a 6Li-loaded plastic scintillator is presented. Existing capture-gated thermal neutron detection techniques were evaluated with the 6Li-loaded plastic scintillator studied in this work. Using simulations and experimental work, shortcomings in its performance were highlighted. As a result, it was proposed that by separating the combined fast and thermal neutron events from gamma events, using established pulse shape discrimination techniques, the thermal neutron events could then be assayed. Experiments were conducted at the National Physical Laboratory, Teddington, performing neutron assays with seven different neutron fields using the proposed technique. For each field, thermal and fast neutron content was estimated and were shown to corroborate with the seven synthesised fields.